The present invention relates to a process and apparatus for forming detergent bars and detergent bars formed thereby. The detergent bars can be of the personal or fabric wash type.
Detergent bars are conventionally manufactured by one of two methods; (i) milling followed by extrusion (xe2x80x9cploddingxe2x80x9d) and stamping (sometimes referred to as the xe2x80x9cmillingxe2x80x9d process), or (ii) casting.
In the milling process, a preformed solid composition comprising all components of the bar is typically plodded, i.e. extruded through a nozzle to form a continuous xe2x80x9crodxe2x80x9d which is cut into smaller pieces of predetermined length, commonly referred to as xe2x80x9cbilletsxe2x80x9d. These xe2x80x9cbilletsxe2x80x9d are then fed to a stamper or, alternatively, are given an imprint on one or more surfaces using, for example, a die of the same dimensions as the bar surface which is hit with force such as with a mallet or a die in the shape of a roller, or simply cut.
There are several shortcomings associated with the milling method of detergent bar manufacture.
A problem encountered with the stamping process is die-blocking, in which amounts of residual detergent left on die halves build up during continued use of the dies. Die blocking can lead to poor or even non-release of the bars from the die surface and/or visible imperfections on the bar surface. Extrusion and stamping also require that the extruded billet be in a substantially xe2x80x9crigidxe2x80x9d form at the process conditions. Die blocking and xe2x80x9csoftxe2x80x9d billets may be caused by soft detergent compositions, for example compositions containing a large proportion of ingredients which are liquid at processing conditions, and/or may also be a result of the shear and extensional forces to which the detergent composition is subjected by the milling process, e.g. the extrusion and/or stamping.
Milling is therefore only suitable for formulations which are plastic and yet which are not soft or do not become soft or sticky due to the shear degradation at operating temperatures of the manufacturing equipment, typically in the range of ambient xc2x130xc2x0 C.
Milled bars also tend to have an oriented structure, aligned along the axis of extrusion. They also tend to form cleavage planes within the bar, which weaken the bar and, with the repeated wetting and drying of the bar in use, can lead to wet-cracking along the planes. Wet-cracking is highly undesirable being both unsightly and leading to bar fracture.
The other conventional method for the manufacture of detergent bars is casting. In casting, detergent compositions in a heated mobile and readily pourable state are introduced into the top of an enclosed cavity (i.e. a mould) of the desired shape and the temperature of the composition reduced until it solidifies. The bar can then be removed by opening the mould.
In order to be castable, the detergent formulation must be mobile and readily pourable at the elevated temperatures employed. Certain detergent formulations are viscous liquids or semi-solids at commercially realistic elevated temperatures and therefore do not lend themselves to casting.
Furthermore, in the casting process, the detergent melt tends to cool slowly and unevenly. This can lead to unwanted structural orientations and segregation of ingredients. Often some sort of active cooling system is employed in order to achieve acceptable processing times. Even when a cooling system is employed, cooling is still generally uneven through the detergent composition in the mould.
A major problem with the casting process is that detergent compositions in the moulds tend to shrink as they cool. This is highly undesirable as the mould is intended to impart a distinctive shape on the bar and/or a logo of some kind. Shrinkage can take the form of dimples, wrinkles or voids, or a depression at the fill point of the bar.
Therefore, there is a need for a process and apparatus for forming detergent compositions into good quality bars (i.e. bars, for example, of good appearance and physical characteristics) which overcomes the identified problems and disadvantages associated with the milling process, and which also avoids the problems associated with casting.
U.S. Pat. No. 2,987,484 (Procter and Gamble) discloses a closed die moulding process in which a basically non-soap fluid mixture of synthetic detergent and a binder-vehicle is rapidly injected through a small orifice into a substantially closed die, the fluid mixture being capable of solidifying into a shape-sustaining form.
The process involves heating the composition to a temperature in the range 70xc2x0 C. to 150xc2x0 C. so that the composition melt is in a fluid-injectable state. In all the examples, the temperature is in the range 82-150xc2x0 C. The melt is circulated through a continuous injection circuit comprising a crutcher in which the fluid mixture is mixed and heated, a pipeline in a loop with the crutcher, a heat exchanger in the pipeline to stabilise the temperature of the melt, and a pump to maintain the circulating and injection pressure.
The viscosity of the heated melt at the conditions of injection is 2-50 Pa.s. This is described as being dependent on the intensity or shear and the temperature and a function of the composition. However, no specific shear rates are given for this viscosity range. A melt having a viscosity in the range 2-50 Pa.s at injection conditions is described as being thick enough so as not to splash in the mould, entrap air or run out of the mould air vents, whilst being thin enough to to permit complete filling of the mould prior to solidification of any composition therein and to avoid excessive injection pressures. Suitable injection pressures range from about 1-20 psi, but are preferably in the range 2-10 psi. In all the examples, the injection pressure is between 5-8 psi. Pressures which are too high are described as causing splashing in the mould and as increasing the density of the melt.
U.S. Pat. No. 2,987,484 also teaches, and it is an essential feature of the claims, that for the process to work, the fluid mixture must be cooled through a nigre (isotropic liquid) plus crystals phase. Furthermore, it is taught that detergent fluid mixtures in the neat or middle (anisotropic liquid) phases are not suitable for closed die moulding because of the excessive viscosity of these phases and the tendency for undesirable complexes to form in these phases. In addition, U.S. Pat. No. 2,987,484 states that successful closed die moulding necessitates avoidance of cooling through neat and middle phases (column 4, lines 8 to 27).
U.S. Pat. No. 2,989,484 is described as overcoming the problems associated with conventional methods of bar manufacture and in particular those associated with milling. However, the solution described has several inherent drawbacks, most of which are common to the casting and framing processes. It is very energy intensive, energy being required to heat the detergent compositions to the high temperatures at which the fluid mixture is injected and subsequently to cool the moulds in order to reduce the solidifying times to acceptable levels. Furthermore, by injecting the compositions as high temperature fluids, the process leads to problems with shrinkage the bars as they solidify. It also fails to address the problem of segregation of ingredients as the detergent composition cools in the mould. The detergent composition in the apparatus is permanently sheared by being pumped through pipes or by a mixer in the crutcher.
Conventional processes of detergent bar manufacture operate either by structuring the detergent composition totally within the mould, requiring initial high heat energy input (e.g. casting), or structuring the detergent composition totally outside the mould/bar-shaping means, resulting in the processing of a rigid solid material prior to moulding (e.g. extrusion and stamping). The latter type of process subjects the structured material to high shear energy (e.g. in stamping). In attempting to overcome the shortcomings of such processes, and in particular those of the milling and framing processes, the process described in U.S. Pat. No. 2,987,484 does not deviate from this general patternxe2x80x94there is a high energy input in terms of the relatively high temperatures used. From this perspective, U.S. Pat. No. 2,987,484 merely provides an alternative casting process in which the detergent material is injected, rather than being poured, into a mould.
The present inventors have found that the problems present in the methods of the prior art can be overcome by operating in a processing window whereby structure is developed partially outside and partially inside the mould. In this way, any disruptive shear effects present in the process will only act on a partially-developed structure and sufficient structure can form in the mould to produce good quality bars. In this way, the structuring of the detergent composition is damaged to a much lower degree during bar formation and higher injection pressures can be tolerated, without disrupting the partial structure.
By partially structuring a detergent composition prior to delivering it to a mould in an injection moulding process, good quality bars can be obtained and the problems of shrinkage, oriented structure and segregation of ingredients are significantly reduced. In addition, production benefits such as shorter bar release times are also achievable.
Thus, according to a first aspect, the present invention provides a process for forming detergent bars comprising applying pressure to a detergent composition to deliver the detergent composition to a mould characterised in that the detergent composition is at least partially structured when it enters the mould.
Preferably, it is the continuous phase of the detergent composition that is at least partially structured.
In the present invention, detergent compositions are considered to be at least partially structured if they contain molecular structure which will affect the viscosity properties of the detergent composition. Additionally or alternatively, detergent compositions may be considered to be at least partially structured if they contain a structuring agent which increases the viscosity of the detergent composition.
Preferably, the detergent composition is in a semi-solid state when delivered to the mould.
In a second aspect, the present invention provides a process for forming detergent bars comprising applying pressure to a detergent composition to deliver the detergent composition to a mould characterised in that the pressure at the point at which the detergent composition enters the mould is greater than 20 psi for at least part of the time over which the detergent composition is entering the mould.
In a third aspect, the present invention provides a process for forming detergent bars comprising applying pressure to the detergent composition to deliver the detergent composition to a mould characterised in that the detergent composition is at a temperature below 70xc2x0 C. when entering the mould.
By delivering the detergent composition to the mould at a lower temperature than that described in the prior art, the process is less energy intensive and the bars cool to a temperature at which they are sufficiently solid to be ejected from the mould more quickly.
The present inventors have designed apparatus for forming detergent bars by injection moulding. More particularly, the present inventors have provided a means for feeding detergent composition to the means for applying pressure.
Thus, the present invention provides an apparatus for forming detergent bars comprising a means for applying pressure to a detergent composition to deliver the detergent composition to a mould and a substantially separate means adapted for feeding detergent composition to the means for applying pressure.
The detergent composition may be introduced into the means for feeding in any suitable state, such as, for example, fluid, semi-solid or particulate form.
We have discovered that a particularly effective means of feeding detergent compositions, including compositions supplied in a fluid state, in an injection moulding process is provided by means of screw extruders.
Thus, the feeding means preferably comprises a screw feeder.
In another aspect, the present invention provides detergent bar obtainable by the process of the present invention.
We have found that the process of the invention is well suited for incorporating additive or benefit agents which are immiscible with the detergent composition. Accordingly, the present invention provides detergent bars obtainable by the process of the present invention comprising a detergent composition and components immiscible with the detergent composition, wherein the immiscible component is present in non-spherical domains.
In a further aspect, the present invention provides for a method for incorporating an additive or benefit agent into a detergent bar, comprising adding the additive or benefit agent to a detergent composition which is at least partially structured and applying a pressure to the detergent composition containing the additive or benefit agent so as to deliver it to a mould.
In a preferred embodiment, the additive or benefit agent is immiscible with the detergent composition.
Unless specified more generally, references herein to the invention or to any preferred features apply to all aspects of the invention.
By xe2x80x9cdetergent barxe2x80x9d is meant a tablet, cake or bar in which the level of surface active agent, which comprises soap, synthetic detergent active or a mixture thereof, is at least 5% by weight based on the bar. The detergent bar may also comprise benefit agents for imparting or maintaining desirable properties for the skin. For example, moisturising agents may be included.
The detergent compositions may comprise homogeneous components or mixtures of components, or may comprise material suspended or dispersed in a continuous phase.
Detergent compositions to be delivered to the mould can be in any form capable of being delivered to the mould. For example, the composition may be in a substantially fluid (e.g. molten, molten dispersion, liquid), substantially semi-solid or substantially solid form, so long as the composition is sufficiently plastic to allow the pressure applying means to deliver it to a mould as would be understood by the person skilled in the art.
Structure
The detergent composition should be compared with a detergent composition which is at the same temperature as the detergent composition under consideration and of substantially the same composition, except for having no structure and/or structuring agent present, whereby it can be ascertained whether viscosity is increased.
Structure can be provided, for example, by liquid crystal formation, a polymeric structuring agent or clay, or a sufficient volume of a dispersed solid component which will affect the viscosity. A solid component can provide structure by interacting to form a network within the detergent composition or through the simple physical interaction/contact of the solid particles with one another or with the continuous phase.
With regards to detergent compositions, and in particular detergent compositions in a substantially fluid or liquid state, there are two general and separate classes of compositions, those with structurally isotropic phases and those with structurally anisotropic phases. Those phase states that are structurally isotropic are liquid, cubic liquid crystal phases and cubic crystal phases. All other phases are structurally anisotropic.
Structured liquids can be xe2x80x9cinternally structuredxe2x80x9d, whereby the structure is formed by primary ingredients, preferably by surfactant material (i.e. anisotropic or having liquid crystal phases), and/or xe2x80x9cexternally structuredxe2x80x9d whereby a three dimensional matrix structure is provided by using secondary additives, for example, polymers (e.g. Carbopols), clay, silica and/or silicate material (including in situ formed aluminosilicates).
Such secondary additives may be present at a level of 1-10% by weight of the detergent composition.
The existence of internal structure in the detergent composition may be due to the components used, their concentration, the temperature of the composition and the shear to which the composition is being or has been exposed.
In general, the degree of ordering of surfactant containing systems increases with increasing surfactant and/or electrolyte concentrations. At very low concentrations of surfactant and/or electrolyte, the surfactant can exist as a molecular solution, or as a solution of spherical micelles, both of these solutions being isotropic, i.e. they are not structured. With the addition of further surfactant and/or electrolyte structures of surfactant material may form. Various forms of such structures exists, e.g. bilayers. They are referred to by various terms such as rod-micelles, anisotropic surfactant phase, planar lamellar structures, lamellar droplets and liquid crystalline phases (most of which are anisotropic but which may be isotropic). Various examples of fluid compositions which are internally structured with surfactant material are given in H. A. Barnes, xe2x80x9cDetergentsxe2x80x9d, Ch.2. in K. Walters (Ed), xe2x80x9cRheometry: Industrial Applicationsxe2x80x9d, J. Wiley and Sons, Letchworth 1980. Often different workers use different terminology to refer to structures which are really the same. For example, lamellar droplets are called spherulites in EP-A-0151884.
The presence of such internal structuring, ordering or anisotropy may be typically revealed by the temperature/viscosity/shear profile of the composition in a manner known to the person skilled in the art. Frequently, the presence of molecular structure gives rise to non-Newtonian fluid behaviour.
The presence and identity of a surfactant structuring system in a detergent composition may be determined by means known to those skilled in the art for example, optical techniques, various rheometrical measurements, X-ray or neutron diffraction, and sometimes, electron microscopy.
As will be known to the person skilled in the art, molecular structure may be detected by the use of polarised light microscopy. Isotropic phases have no effect upon polarised light, but structured phases will have an effect upon polarised light and may be birefringent. An isotropic liquid would not be expected to show any kind of periodicity in X-ray or neutron diffraction micrographs, whereas molecular structure may give rise to first, second or even third order periodicity, in a manner which will be known to the person skilled in the art.
Preferably, the detergent composition is in a semi-solid state when delivered to the mould. A detergent composition may be considered to be in a semi-solid state if sufficient structure is present in the composition so that it no longer behaves like a simple liquid, as would be understood by the person skilled in the art.
Contrary to the prior art, we have found that it is possible to obtain detergent bars having good physical properties by cooling a detergent composition from or through a neat and/or middle liquid crystal phase. Furthermore, we have found that it is not essential for the detergent composition to be cooled through a nigre plus crystals phase in order to achieve successful bar formation by an injection moulding process.
Accordingly, the detergent composition entering the mould preferably cools from and/or through an anisotropic liquid crystal phase.
The processes and apparatus of the present invention therefore provide a means for producing good quality detergent bars from detergent formulations which do not lend themselves to the milling or casting methods of manufacture, for example, formulations, in particular personal wash formulations, which have a high concentration of ingredients in a liquid state at ambient conditions, formulations which have a shear-sensitive solid structure, and formulations which are too viscous to cast.
One of the benefits provided by the present invention is a reduction in the problems associated with shrinkage of the bar in the mould as the bar cools. This results in greater accuracy in replication of the surface contours and form of the cavity. In particular, good logo reproduction can be obtained.
In order to overcome the problems associated with the process of the prior art, the detergent compositions of the present invention are typically more viscous than those of the prior art. Consequently, the pressure required to deliver a detergent composition to a mould is greater.
Pressure
The pressure applied to the detergent composition in contact with the pressure applying means is referred to herein as the xe2x80x9capplied pressurexe2x80x9d, and references to xe2x80x9capplyxe2x80x9d and xe2x80x9capplyingxe2x80x9d pressure to a detergent composition refer to the applied pressure. As the detergent composition may be relatively viscous, the pressure experienced by the composition further down the flow path may be lower.
xe2x80x9cInjection pressurexe2x80x9d is the pressure on the detergent composition at the point of entering the mould.
The inventors have discovered that higher pressures than those of the prior art can be used to deliver a detergent composition to a mould without compromising the final molecular structure of the detergent bar. As in the second aspect of the invention, use of injection pressures in excess of 20 psi can allow relatively viscous compositions to be fed to a mould.
Applied pressures may be in the order of 10-50 psi. However, higher applied pressures, for example up to 1000 psi, may be used to deliver relatively viscous (e.g. semi-solid) detergent compositions to the mould. The applied pressure will typically not exceed 750 psi, and more typically not exceed 500 psi. Excessive shear can be avoided at such pressures by controlling process parameters such as temperature, flow rate and apparatus design.
The injection pressure is typically greater than 20 psi, preferably greater than 29.4 psi, and more preferably greater than 50 psi. Because the detergent compositions being injection moulded are at least partially structured and/or at relatively low temperatures, significantly higher injection pressures than those reported in U.S. Pat. No. 2,987,784 may have to be employed. For example, the detergent composition may be in a substantially semi-solid form. Injection pressures greater than 200, greater than 400, and even after than 700 psi may be used.
We have found that the problems associated with bar shrinkage in the mould may be reduced, if there is a need to do so, by delivering further detergent composition to the mould as the volume in the mould cools or becomes solid. To achieve this a xe2x80x9cholding pressurexe2x80x9d is placed on the detergent composition in the mould. In this manner the total volume in the mould can be maintained and shape reproduction further improved.
Furthermore, use of a xe2x80x9cholding pressurexe2x80x9d minimises weld lines (i.e. interfaces between flow fronts of detergent material inside the mould) and improves logo definition.
Thus, it is possible to obtain detergent bars with reduced shrinkage and having good physical properties by applying a pressure to a detergent composition to deliver the detergent composition to a mould and continuing to apply the pressure on the detergent composition for a period after the mould has been filled.
The pressure created in the mould by continuing to apply pressure to a detergent composition entering a mould after the mould has been filled is herein referred to as the xe2x80x9cholding pressurexe2x80x9d. The detergent compositions may be subjected to high holding pressure within the mould. For example, such pressures may be up to 1000 psi.
All pressure figures are psi gauge (psig), i.e. the level above or below atmospheric pressure.
The time over which a xe2x80x9cholding pressurexe2x80x9d is developed by continuing to apply pressure to the detergent composition after the mould has been filled is referred to herein as the xe2x80x9cholding timexe2x80x9d. The holding time will vary depending on the properties of the detergent composition being delivered to the mould. For example, compositions being delivered to a mould in a molten state and at high temperatures may need a longer holding time than compositions which are delivered to a mould in a semi-solid state and/or at a lower temperature.
Typically, the holding time is less than 2 minutes, preferably less than 1 minute, more preferably less than 30 seconds, and most preferably less than 10 seconds. The holding time may be very short, for example, less than 1 second.
Temperature
The inventors have discovered that detergent compositions at lower temperatures than those typically employed by the prior art can be delivered under pressure to a mould without compromising the final molecular structure of the detergent bar. Where the presence of structure in a detergent composition to be delivered to the mould can be clearly identified, it may be acceptable to have the detergent composition at a temperature of 100xc2x0 C. or more when it enters the mould. However, as in the third aspect of the invention, a detergent composition can be delivered a mould under pressure to a mould at a temperature of less than 70xc2x0 C. when entering the mould. Excessive shear can be avoided at such temperatures by controlling process parameters such as flow rate and apparatus design.
Detergent compositions do not usually have a simple melting point, but pass instead from a solid form, to a semi-solid form and then to a fluid (or molten) form as the temperature increases. Any practical detergent composition in bar form will be in a substantially solid state at ambient or normal storage and/or use temperatures, which are normally in the range up to 30-40xc2x0 C.
Accordingly, the detergent composition preferably enters the mould at a temperature above ambient, e.g. preferably above 30xc2x0 C., more preferably above 40xc2x0 C.
Of course, the lower the temperature, the less energy is required to heat the composition from the ambient, the more quickly the bar cools and the less the tendency for the bar to shrink.
It is a particular advantage of the present invention that the detergent composition can enter the mould at a lower temperature than in a simple casting technique. When heating solid detergent compositions, less heat (i.e. energy) may be required as the operating temperatures can be lower. When cooling liquid detergent, no heating may be required at all. The present invention therefore offers economy in operation.
Typically, the detergent composition may be at a temperature of 60xc2x0 C. or less.
The present invention is particularly suited to detergent compositions which undergo supercooling, i.e. thermal energy can be removed outside the mould without the final bar structure forming.
Injection Moulding Apparatus
Injection moulding is a process which is presently particularly used in the moulding of synthetic polymeric thermoplastic articles, particularly thermoplastic articles having thin cross sections and complex shapes.
In essence, an injection moulding apparatus for plastic material comprises a substantially closed mould and a means for delivering the plastic material under raised pressure into the substantially closed mould. Preferably there are means for raising the temperature of the plastic material to a temperature where the material is flowable under pressure. The process of the present invention can be carried out using such known injection moulding apparatus, with or without any means for heating the feed. Preferred modifications according to the present invention are discussed below.
Detergent compositions of the present invention may be injection moulded using an apparatus comprising a means for applying pressure to the detergent composition so as to drive the detergent composition into a mould. A xe2x80x9cmeans for applying pressurexe2x80x9d is defined as a device capable of containing a material and of applying a pressure to that material so as to force it into a mould.
Suitable types of apparatus that lend themselves to driving detergent composition into a mould include positive displacement pump-type arrangements such as, for example, piston pump (which can include extruders), gear pump and lobe pump-type arrangements.
A suitable apparatus is a simple ram extruder in contact with a mould. Such apparatus typically comprises a reservoir or barrel for the detergent composition, a plunger for applying pressure to the material in the reservoir and an exit port through which the detergent composition is driven, directly or indirectly, into a mould. Simple ram extruder apparatus is particularly suited to injection moulding of detergent compositions in, for example, a semi-solid form.
Injection moulding apparatus as described above may be used for the processes of the invention.
In a preferred embodiment, the detergent composition is preferably at least partially structured when delivered to the mould. Preferably, the detergent composition is in the semi-solid form when delivered to the mould. Of course, the present invention also provides for detergent compositions to be injection moulded in a substantially fluid form.
Some detergent compositions may be made permanently sticky if they are injection moulded under the wrong conditions. That is, some solid detergent compositions have a complex molecular structure which may be disrupted if the solid is exposed to excessive shearing stresses. The molecular structure may not be re-established after such shearing, so that the detergent composition will remain in a sticky, unusable state.
It is accordingly desirable to ensure that such detergent compositions are not exposed to excessive shear during delivery to the mould.
In order to control the shear to which the detergent composition is subjected, the nature of the detergent composition itself needs to be taken into account, in particular its viscosity and molecular structure at various temperatures. To control the shear, one can control process parameters such as the temperature, pressure applied to the composition, flow rate of detergent composition in the apparatus and configuration of the apparatus. Configurations such as severe bends, constrictions and fast moving parts may subject the detergent composition to high shear.
It has been found that by delivering the detergent composition at an appropriate temperature to the mould, the shear-sensitive structure may not be fully formed and the structure of the composition at room temperature is not lost. Any suitable method may be used to control the temperature of the detergent composition being injected into the mould. It may be supplied at a temperature suitable for delivery to the mould and require no alteration to its temperature. Alternatively, and preferably, the temperature of the detergent composition is altered before or whilst it is fed to the mould by using heating or cooling means to raise or lower the temperature of the composition as is appropriate.
Preferably, the state of the detergent composition is altered before or whilst it is fed. For example, it may pass from a liquid phase to a semi-solid state. Alternatively, it may pass from a solid to a semi-solid state.
Any suitable cooling or heating means may be applied to the injection moulding apparatus in which the detergent composition is contained/passes during the injection moulding process.
Suitable heating and cooling means are well-known to the skilled person in the art. For example, a suitable cooling means is a cooling jacket containing a cooling medium, and suitable heating means include, for example, electrical heating jackets containing a heating medium or heat exchangers of various forms.
A high temperature may be maintained near the point at which detergent composition is fed into the mould, so as to prevent blockage due to solidification.
A plurality of separately controllable heating means or cooling means may be provided at different positions in the apparatus. A stepped temperature profile can then be provided in the direction of flow of detergent composition. For example, the temperature may increase or decrease in steps.
Detergent compositions often come in solid particulate forms (e.g. pellets) which are then either extruded and stamped in a milling process, or, melted and cast in a casting process. Known injection moulding apparatus used in the plastics industry normally uses particulate plastic starting material which flows easily from a hopper. In contrast, detergent compositions in particulate form may be sticky and flow relatively poorly. Therefore special means may be required in order to ensure good feed of detergent composition to the apparatus.
The inventors have also observed that some detergent compositions are produced and supplied in a high temperature, molten state. Therefore means for feeding liquid detergent composition to the means for applying pressure to the detergent composition will be required.
Accordingly, the present invention provides an apparatus for forming detergent bars comprising a means for applying pressure to a detergent composition to deliver the detergent composition to a mould and a substantially separate means adapted to feed detergent composition to the means for applying pressure to the detergent composition.
The feeding means are substantially separate in that no parts of the feeding means have any significant role in applying pressure to the detergent composition. Of course, the feeding means is suitably in fluid connection with the means for applying pressure to the detegrent composition, whereby the detergent composition maybe readily fed into the means for applying pressure.
Examples of suitable feeding means include a conveyor, a container with a tapering lower section, an agitator, a ram feeder, a screw feeder or any number thereof in any combination.
In a preferred embodiment, the detergent composition is supplied to the feeding means in a substantially solid (e.g. particulate) or semi-solid form. xe2x80x9cParticulate formxe2x80x9d encompasses pellets, flakes, noodles, granules and chips as are well-known in the art.
Where a detergent composition is supplied in a substantially solid form, a heating means may be required to heat the material in the apparatus (e.g. in the reservoir in the case of a ram extruder apparatus) so that it becomes and/or remains flowable under pressure.
If the detergent composition is provided in a substantially fluid form, then a cooling zone may be employed instead of or in addition to a heating zone. If the molten feed is supplied at a temperature above 70xc2x0 C., it is preferably cooled prior to being delivered to the mould. Of course, it is understood that detergent compositions may be introduced into the mould at temperatures greater than 100xc2x0 C. Furthermore, a heating apparatus may be used to maintain such a high temperature.
It is preferred feature of the feeding means that it is capable of supplying a continuous feed of detergent composition.
The means for feeding detergent material may feed the composition to the means for applying pressure or to a zone preceding the means for applying pressure such as a heating or cooling zone. In a preferred embodiment, the means for feeding detergent material feeds the composition into an accumulator zone which provides a interface between the continuous operation of the feeder and the discontinuous injection cycle of the pressure applying means.
Means for controlling the temperature of the detergent composition may be provided at any position in the injection moulding apparatus. For example, such heating or cooling means may be provided in the means for applying pressure, in the feeding means or in a separate zone, or in any combination thereof. A separate heating zone may be placed, for example, between the means for feeding detergent material and means for applying pressure.
The present invention provides for the use of screw extruders as part of the injection moulding apparatus, either as the feeding means, pressure applying means or both. In a reciprocating injection moulder, the means for applying pressure to the prepared (e.g. thermally heated) material is provided by the screw itself. Typically, the screw is movable along its axis away from the mould. As flowable material is delivered into the accumulation zone at the end of the screw barrel, the pressure generated there is allowed to push the screw back. In order to apply the pressure to the accumulated molten material (the xe2x80x9cshotxe2x80x9d), the screw is forced (usually using hydraulic pressure) forwards towards the accumulation zone thereby placing pressure on the material there, which moves through a nozzle into the mould. A check valve or specially designed screw tip prevents material flowing back into the screw flights.
The means for applying pressure to the detergent composition may comprise the tip of a screw extruder, as described above for known injection moulding apparatus. Alternatively, separate means for delivering detergent under pressure may be used, as set out below.
Preferably, the means for feeding detergent composition comprises a feeder in the form of a screw feeder. This is found to give particularly smooth feed.
Screw geometry may be designed to suit the formulation being processed. The rotational speed of the screw or screws is controllable to provide an acceptable flow rate of material to the accumulation zone or means for applying pressure, without applying unacceptable shear to the detergent.
There are particular problems with fluid detergent compositions. Single screw extruders rely on drag flow for conveying, and therefore to convey fluids they need to be specifically designed with a close clearance and/or inclined so that gravity aids the forward flow of material. It is accordingly preferred to have two parallel screws with intermeshing, preferably self-wiping flights which provide positive displacement to propel detergent composition forwards. The screws may rotate in opposite directions (counter-rotating) but are preferably co-rotating to reduce the reverse pressure flow. Such twin-screw extruders with intermeshing flights for delivering liquids or solids are known to the skilled person.
It may be preferable not to employ a displaceable screw to apply pressure to the detergent composition to deliver it to the mould. Instead, a pressure chamber may be provided, where material can accumulate, comprising at least one wall defined by a piston which is movable to increase or decrease the volume of the pressure chamber, and at least one injection nozzle.
In a preferred embodiment, the screw extruder, in addition to feeding material for injection moulding into the means for applying pressure, will also perform the function of preconditioning the material to a desired physical state for injection. By providing the screw extruder with one or more heating and/or cooling zones, and by selecting, for example, appropriate screws, screw alignment and screw speed, the material fed into the extruder can be intimately mixed and structured to whatever extent is required for the particular injection moulding process being used and product characteristics sought. For example, a preferred embodiment of the present invention is that material be injected in a substantially semi-solid state.
In addition, the feeding means, preferably a screw extruder, can contain intermediate ports for degassing and/or for adding further ingredients. Additives, such as, for example, dyes and fragrances and other benefit agents can also be added through intermediate ports along the length of the screw feed.
Using a screw feed with a temperature profile, it is possible to add ingredients and/or additives and/or benefit agents to the bulk flow of material in the feeder at a specific temperature. In addition, the material in the screw feed can be mixed and/or structured to a greater or lesser extent as is moves within the screw feed depending on the equipment and process parameters employed. It is thus possible to add ingredients and/or additives and/or benefit agents to the bulk flow of material when it is at a chosen level of viscosity and/or mixing and/or structuring.
Furthermore, it is also possible for soap formation (e.g. saponification) or non-soap detergent surfactant formation (e.g. neutralisation of anionic surfactant acid precursors) to take place within the screw extruder, more particularly the first part of the screw extruder.
In addition to degassing, gas (e.g. air) can also be added to the detergent composition to be injection moulded in order to produce, for example, reduced density or floating bars. Preferably, gas would be added in the screw extruder stage.
Injection Nozzle
The means for applying pressure to the detergent composition may be connected to the mould by a simple passage, or a passage having non-return means or connections for bypass ducts, to allow quick withdrawal of the pressurizing means after the mould is filled and smooth operation of the apparatus.
In a preferred embodiment, however, the detergent composition is fed through a nozzle whose length is a significant proportion (at least half, preferably at least three quarters) of the length of the internal volume of the mould. It has been found that there can be a problem in simple filling with jetting or xe2x80x9csnakingxe2x80x9d of the material in the mould. By providing a nozzle which extends substantially to the distant end of the mould, good fill has been found to be possible. Preferably, the nozzle and mould move relative to each other whilst the detergent composition is being supplied. The mould may be moved with respect to the means for applying pressure and/or the nozzle may be moved with respect to the mould whilst the detergent composition is being supplied. The rate at which the nozzle and mould move relative to each other is preferably matched to the rate of detergent delivery so that the nozzle remains just below the surface of detergent composition in the mould. This has been found to give particularly good fill. In a preferred embodiment, the nozzle is moved with respect to the mould.
The nozzle may be heated or pre-heated in order, for example, to prevent any of the detergent composition solidifying (depositing) in the nozzle and thus inhibiting smooth delivery of the composition to the mould.
Preferably, the diameter of the injection nozzle for use with the means for delivering detergent composition under pressure is small. Preferably the diameter is in the range 1 to 20 mm, preferably 5 to 10 mm, most preferably about 8 mm in diameter and of circular section.
Mould
The mould of the present invention may be constructed of any suitable material, for example a rigid material with good mechanical strength. Where rapid cooling is desired, a material with high thermal conductivity may be preferred. Preferably the mould comprises a material selected from metals and their alloys (for example, aluminium, brass and other copper alloys, steels including carbon and stainless steel), sintered forms of metals or metal composites, non-metallic materials such as ceramics, composites, and thermosetting plastics in porous or foamed forms.
Moulds may comprise rigid and non-rigid materials, for example, non-rigid plastics may be employed. The mould may form part or the whole of the packaging of the detergent bar product. In this respect, the packaging may be of a rigid nature or it may be non-rigid, e.g. a wrapper. For example, the inner lining of a rigid mould may comprise a xe2x80x9cwrapperxe2x80x9d for the detergent bar product so that a wrapped bar is released from the mould. The mould may also comprise an expandable lining within a cavity defined by the mould, the lining expanding to fill the cavity as detergent composition is delivered to the mould. Such linings and wrappers that may be released with the bar may be integral parts of the product packaging or may be removed once the bars are released, e.g. they may merely be used to facilitate easy release of the bars from the mould.
The mould may be pre-cooled or preheated prior to delivery of detergent composition to the mould. The internal surface of the mould may be preheated to a temperature, for example, in excess of the delivery temperature and/or the melt temperature of the composition. Such preheating of the mould has been found to provide for a smoother, more glossy finish to the bars.
After delivery of detergent, the mould may be cooled to encourage rapid solidification of the detergent. Any suitable coolant may be used, e.g. air, water, ice, solid carbon dioxide or combinations thereof, depending on the speed of cooling and the end temperature required. Preferably, at least part of the external face of the mould is provided with a means to improve cooling efficiency of the mould after injection. In preferred embodiments of the invention, such means comprise fins or ribs for air cooling or jackets for circulation of a coolant liquid.
The mould suitably comprises at least two rigid complementary dies adapted to be fitted to each other and withstand the injection and holding pressure, each die corresponding to a respective portion of the desired shape of moulded article, said dies when in engagement along the contacting portion of their rims defining a cavity corresponding to the total shape of the moulded article. The use of multiple part moulds comprising at least two die parts allows for the manufacture of highly diverse 3-dimensional shapes; for example circular, oval, square, rectangular, concave or any other form as desired.
In a mould comprising at least two die parts, at least one of said dies may be provided with a sealing means along the contacting portion of the rim thereof. More preferably, said sealing means comprises an elastomeric gasket.
The mould is provided with an internal surface, the size and shape of which may vary depending on the form of the final product. The internal surface of the mould may be coated in part or in total with a material having good release characteristics, such as low surface energy, or other properties, as described for instance in WO97/20028. Examples of such materials include fluoroplastics and fluoropolymers, silicones, and other elastomeric materials. The thickness of the coating is preferably less than 1 mm, more preferably less than 50 microns. The internal surface of the mould may be flat, concave or convex or any-other shape as desired. The shape may be such as to accommodate bar shrinkage without detracting from the final bar appearance, e.g. very convex surfaces can be used.
The internal surface of the mould is optionally provided with mirror images of inscriptions or logos or figures desired on the surface of the moulded article, either as projections or depressions.
To ensure easy detachment of the article from the mould without distortion or damage to the inscription on the article the inscription may be designed such that the rim of the mirror image of the inscription is not exactly perpendicular to the die surface, but is appropriately beveled. To further prevent distortion or damage to the inscription or logo or figure, the finish on the inner die surface should be free from burrs and blemishes and preferably be carefully polished.
Leakage of material from moulds comprising die parts may be prevented by having the joining surfaces of the dies closely matching, e.g. by lapping or by providing a gasket. In the case of high viscosity materials, flat face contact is sufficient. The two dies are held together by the use of nuts and bolts or by some sort of clamping mechanism, for example a hydraulic mechanism. Alternatively the external surfaces of the die parts can slide on inclined planes into a separate housing means which enables the mould to withstand lateral forces. It is important that good seals are achieved when high applied and holding pressures are being used.
Typically, the mould has a xe2x80x9cgatexe2x80x9d, this being the opening in the mould through which detergent composition may be delivered to the mould cavity. In this respect, the gate opens on one side to the mould cavity and on the other side may be engaged directly or indirectly to the pressure applying means.
The detergent composition may be delivered from the pressure applying means via a runner (or sprue) channel. In this respect, it may be beneficial to heat or cool the runner channel. The detergent composition may be delivered to the mould cavity directly without any runner channel. For example, it may be delivered directly through a nozzle.
The mould may comprise a xe2x80x9cneckxe2x80x9d, a short channel separated from the mould cavity by the gate. The detergent composition may be delivered through the mould neck. Alternatively, a nozzle may enter the mould cavity via the neck and gate in order to deliver the detergent composition.
In a mould comprising die parts, the gate and/or a neck may be totally present in one die part or may be formed on the engagement of two or more die parts. The gate opens on one side to the cavity and on the other side is adapted to be engaged, suitably by means of a nozzle entering the mould via a neck, to the pressure applying means.
The mould may be of such a design that it can be closed once it is full or once the material in the mould has solidified to the extent that an outer shell has formed. By making the mould air tight, shrinkage effects are controlled. In a preferred embodiment, the gate remains open whilst a pressure continues to be applied by the pressure applying means. The mould may be closed at the gate whilst the material inside the mould is still under pressure.
The process may be carried out in a continuous manner by having a plurality of moulds circulating through a feed station where the detergent composition is injected under pressure in to each mould and subsequently taken through the steps of cooling to solidify the material further and demoulding before being recycled again.
In a mould comprising die parts, the die parts may be designed so there is a differential level of adherence of the solidified detergent bars. This allows flexibility in the methods of release of the bars from the moulds as the dies are split. Differential adherence of the solidified bars to the dies may be achieved, for example, by coating certain die parts as described above and not others, or by using coatings with different release characteristics.
Venting
In injection moulding processes it is generally necessary to provide a means for venting, i.e. removal of air from the mould, as the mould is filled. Mould venting is a technique employed in various known injection moulding processes, for example in the thermoplastics industry, and such techniques may also be suitably employed in the present invention as would be understood by the man skilled in the art.
In the present invention, mould venting may be achieved by simply providing a venting means such as, for example, a small hole(s) or a slit(s) in the mould. The vent may be formed by two or more die parts of the mould coming together.
Alternatively, the vent may be an integral part of a mould or die. The vent may be closed by the detergent composition filling the mould being solidified at that point. Alternatively, a small amount of detergent material may exit the mould through the vent, this material being subsequently removed. It is also possible to have a venting means which can be opened and closed, being open during mould filling and closed once the mould has been filled. It is also possible to facilitate air flow from the mould by adopting suitable shapes for the mould and logo.
The present invention also provides for venting by means of incorporating a porous material into the mould. Porous material herein includes any material that is porous or permeable and which has pores within the range of from 2 to 500 microns in diameter. Preferably, the pores are in the range of from 5 to 50 microns, especially from 10 to 20 microns.
The porous material may constitute a part or all of the mould or die part. For example, it may be that just the logo comprises porous material. Moulds comprising porous material can be used for forming bars from detergent compositions delivered in molten and non-molten states.
Suitable porous material for use in the moulds as a venting means is Metapor F100 AL, a microporous, air permeable, aluminum available from Portec, North America, a division of NEST Technologies or from Portec, Ltd. a Swiss company. Another porous die material may be Porcerax II, a porous steel available from Mold Steel, Inc., of Erlanger, Ky., USA. Bar release can also be facilitated by pressurising, for example, a porous die after the mould has been filled and the detergent composition solidified to an appropriate degree.
In a further embodiment, the present invention provides for air present in the mould to be removed by vacuum or partial vacuum during, or more preferably, prior to filling.
In a preferred embodiment of the present invention, the nozzle is adapted with means to allow air to escape from the mould as the nozzle delivers material to the mould. Preferred means are channels running parallel to the nozzle""s length. Such channels suitably extend most of the length of the nozzle, although preferably they do not extend to the very tip of the nozzle. When the nozzle is delivering detergent composition within the mould cavity, air can flow along these channels out of the mould. In a preferred embodiment, the nozzle is withdrawn from the mould cavity as the cavity fills. When the nozzle reaches the point where it is substantially flush with the gate of the mould, the unchannelled portion of the nozzle tip provides an effective air seal. This allows a holding pressure to be applied as required.
Bar Formulations
Suitable detergent compositions for injection moulding include the following ingredients:
(A) 10-60% by weight of a synthetic, non-soap detergent
(B) 0-60% by weight of a water soluble structurant which has a melting point in the range 40-100xc2x0 C.,
(C) 5-60% by weight of a water insoluble structurant which has a melting point in the range 40-100xc2x0 C.,
(D) 1-25% by weight water,
(E) 1-20% by weight total composition one or more amphoteric and/or zwitterionic surfactants,
(F) 0-20% by weight total composition one or more nonionic surfactants,
(G) 0-60% by weight soap,
(H) Other optional ingredients as described below,
(I) 0-10% by weight total electrolyte.
Suitable synthetic detergents for use in the process of the present invention include anionic surfactants such as C8-C22 aliphatic sulphonates, aromatic sulphonates (e.g. alkyl benzene sulphonate), alkyl sulphates (e.g. C12-C18 alkyl sulphates), alkyl ether sulphates (e.g. alkyl glyceryl ether sulphates).
Suitable aliphatic sulphonates include, for example, primary alkane sulphonate, primary alkane disulphonate, alkene sulphonate, hydroxyalkane sulphonate or alkyl glyceryl ether sulphonate (AGS).
Other anionic surfactants that can also be used include alkyl sulphosuccinates (including mono- and dialkyl, e.g. C6-C22 sulphosuccinates), alkyl and acyl taurates, alkyl and acyl sarcosinates, sulphoacetates, alkyl phosphates, alkyl phosphate esters, alkoxyl alkyl phosphate esters, acyl lactates, monoalkyl succinates and maleates, sulphoacetates.
Another surfactant which may be used are the acyl isethionates (e.g. C8-C18). These esters are prepared by reaction between alkali metal isethionate with mixed aliphatic fatty acids having from 6 to 18 carbon atoms and an iodine value of less than 20. At least 75% of the mixed fatty acids have from 12 to 18 carbon atoms and up to 25% have from 6 to 10 carbon atoms. The acyl isethionate may be an alkoxylated isethionate such as is described in Ilardi et al., U.S. Pat. No. 5,393,466, hereby incorporated by reference into the subject application.
The anionic surfactants used are preferably mild, i.e. a surfactant which does not damage the stratum corneum, the outer layer of the skin. Harsh surfactants such as primary alkane sulphonate or alkyl benzene sulphonate will generally be avoided.
Suitable water soluble structurants include moderately high molecular weight polyalkylene oxides of appropriate melting point (e.g., 40 to 100xc2x0 C., preferably 50 to 90xc2x0 C.) and in particular polyethylene glycols or mixtures therefore. Polyethylene glycols (PEG""s) which are used may have a molecular weight in the range 2,000 to 25,000. Also included are water soluble starches.
Suitable insoluble structurants are generally an unsaturated and/or branched long chain (C8-C24) liquid fatty acid or ester derivative thereof; and/or unsaturated and/or branched long chain liquid alcohol or ether derivatives thereof. It may also be a short chain saturated fatty acid such as capric acid or caprylic acid. Examples of liquid fatty acids which may be used are oleic acid, isostearic acid, linoleic acid, linolenic acid, ricinoleic acid, elaidic acid, arichidonic acid, myristoleic acid and palmitoleic acid. Ester derivatives include propylene glycol isostearate, propylene glycol oleate, glyceryl isostearate, glyceryl oleate and polyglyceryl diisostearate.
Examples of alcohols include oleyl alcohol and isostearyl alcohol. Examples of ether derivatives include isosteareth or oleth carboxylic acid; or isosteareth or oleth alcohol. Zwitterionic surfactants suitable for use in formulations are exemplified by those which can be broadly described as derivatives of aliphatic quaternary ammonium, phosphonium, and sulphonium compounds, in which the aliphatic radicals can be straight or branched chain, and wherein one of the aliphatic substituents contains from about 8 to about 18 carbon atoms and one contains an anionic group, e.g. carboxy, sulphonate, sulphate, phosphate, or phosphonate.
Amphoteric detergents which may be used in this invention include at least one acid group. This may be a carboxylic or a sulphonic acid group. They include quaternary nitrogen and therefore are quaternary amido acids. They should generally include an alkyl or alkenyl group of 7 to 18 carbon atoms. Suitable amphoteric detergents include simple betaines or sulphobetaines.
Amphoacetates and diamphoacetates are also intended to be covered in possible zwitterionic and/or amphoteric compounds which may be used.
In addition to one or more anionic and amphoteric and/or zwitterionic, the surfactant system may optionally comprise a nonionic surfactant at a level of up to 20% by weight.
The nonionic which may be used includes in particular the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example aliphatic alcohols, acids, amides or alkyl phenols with alkylene oxides, especially ethylene oxide either alone or with propylene oxide. Specific nonionic detergent compounds are alkyl (C6-C22) phenols-ethylene oxide condensates, the condensation products of aliphatic (C8-C18) primary or secondary linear or branched alcohols with ethylene oxide, and products made by condensation of ethylene oxide with the reaction products of propylene oxide and ethylenediamine. Other so-called nonionic detergent compounds include long chain tertiary amine oxides, long chain tertiary phosphine oxides and dialkyl sulphoxides.
The nonionic may also be a sugar amide, such as a polysaccharide amide. Specifically, the surfactant may be one of the lactobionamides described in U.S. Pat. No. 5,389,279 to Au et al. which is hereby incorporated by reference or it may be one of the sugar amides described in U.S. Pat. No. 5,009,814 to Kelkenberg, hereby incorporated into the subject application by reference.
Other surfactants which may be used are described in U.S. Pat. No. 3,723,325 to Parran Jr. and alkyl polysaccharide nonionic surfactants as disclosed in U.S. Pat. No. 4,565,647 to Llenado, both of which are also incorporated into the subject application by reference.
The nonionic surfactant can also be a water soluble polymer chemically modified with hydrophobic moiety or moieties. For example, EO-PO block copolymer, hydrophobically modified PEG such as POE(200)-glyceryl-stearate can be included in the formulations claimed by the subject invention. Formulations can furthermore optionally contain up to 60% soap made by normal soap making procedures. For example, the products of saponification of natural material such as tallow, coconut oil, palm oil, rice bran oil, fish oil or any other suitable source of long chain fatty acids may be used. The soap may be neat soap or middle phase soap.
In addition, the compositions of the invention may include optional ingredients as follows:
Organic solvents, such as ethanol or propylene glycol; auxiliary thickeners, such as carboxymethylcellulose, magnesium aluminum silicate, hydroxyethylcellulose, methylcellulose, carbopols, glucamides, or Antil(copyright) from Rhone Poulenc; perfumes; sequestering agents, such as tetrasodium ethylenediaminetetraacetate (EDTA), EHDP or mixtures in an amount of 0.01 to 1%, preferably 0.01 to 0.05%; and coloring agents, opacifiers and pearlizers such as zinc stearate, magnesium stearate, TiO2, EGMS (ethylene glycol monostearate) or Lytron 621 (Styrene/Acrylate copolymer); all of which are useful in enhancing the appearance or cosmetic properties of the product.
The compositions may further comprise antimicrobials such as 2-hydroxy-4,2xe2x80x24xe2x80x2trichlorodiphenylether (DP300); preservatives such as dimethyloldimethylhydantoin (Glydant XL1000), parabens, sorbic acid etc.
The compositions may also comprise coconut acyl mono- or diethanol amides as suds boosters, and strongly ionizing salts such as sodium chloride and sodium sulphate may also be used to advantage. Such electrolyte is preferably present and level between 0 and 5% by weight, preferably less than 4% by weight.
Antioxidants such as, for example, butylated hydroxytoluene (BHT) may be used advantageously in amounts of about 0.01% or higher if appropriate.
Cationic conditioners which may be used include Quatrisoft LM-200 Polyquaternium-24, Merquat Plus 3330xe2x80x94Polyquaternium 39; and Jaguar(copyright) type conditioners.
Polyethylene glycols which may be used include Polyox WSR-205 PEG 14M, Polyox WSR-N-60K PEG 45M, Polyox WSR-N-750 PEG 7M and PEG with molecular weight ranging from 300 to 10,000 Dalton, such as those marketed under the tradename of CARBOWAX SENTRY by Union Carbide.
Thickeners which may be used include Amerchol Polymer HM 1500 (Nonoxynyl Hydroethyl Cellulose); Glucam DOE 120 (PEG 120 Methyl Glucose Dioleate); Rewoderm(copyright) (PEG modified glyceryl cocoate, palmate or tallowate) from Rewo Chemicals; Antil(copyright) 141 (from Goldschmidt).
Clays and paraffin wax.
Another optional ingredient which may be added are the deflocculating polymers such as are taught in U.S. Pat. No. 5,147,576 to Montague, hereby incorporated by reference.
Another ingredient which may be included are exfoliants such as polyoxyethylene beads, walnut shells and apricot seeds. The detergent compositions of the present invention may include typical known additives such as perfumes and colourants.
Additives and Benefit Agents
For improving the consumer-perceived properties of the bars, it may be desirable to incorporate benefit agents and/or other additives into the formulation. Skin benefit agents are defined as products which may be included in a detergent composition which will be deposited onto the skin when the detergent composition is applied to the skin and which will impart or maintain desirable properties for the skin.
It is particularly preferred that the detergent compositions used in the present invention comprise benefit agents such as, for example, moisturising components.
Typically, such benefit ingredients are substantially immiscible with the detergent composition and are desired to be present in the form of discrete zones. When the detergent composition is in a fluid state as in a casting process, any density differences between the benefit ingredients and the fluid detergent mixture can lead to phase separation in the unstirred system such as would exist in a mould after casting. The benefit agent may exist as a single component phase or with some of the ingredients of the formulation.
One of the problems associated with benefit agents is that they are washed away by the lathering surfactants before they are deposited on the skin. One way to avoid this is to disperse benefit agents heterogeneously in the bar, e.g. as zones, allowing direct transfer of the benefit agent as the bar is rubbed on the skin. It is widely accepted that more benefit agent deposits on the skin when the benefit agent is dispersed heterogeneously.
Further, in order to give optimum deposition to the skin during the wash process, it may be desirable to control the size of the zones occupied by the benefit ingredient in the finished bar product. In a fluid system, it is difficult to stabilise droplets of a specific size.
Such zones may be of size 1 micron to 5 mm. Preferably, the zones are of size 15 to 500 microns for example as set out in WO 96/02229. More preferably, the zones are of size in the range 50 to 200 microns.
The inventors have found that the process of the invention is particularly suitable for the incorporation of benefit agents to the detergent mixture, and in particular when the detergent mixture is in a semi-solid state. Preferably, benefit agent is added to the detergent composition in the means for feeding the detergent composition. Where the means for feeding the detergent composition comprises a screw feed, the benefit agent may be added at any suitable position along the screw feed. Using the equipment of the present invention, where a temperature profile exists in the equipment, it is possible to choose the temperature at which the benefit agent is added. It is therefore possible to introduce the benefit ingredient into a bulk flow of chosen viscosity. By using appropriate equipment and processing parameters, it is also possible to introduce the benefit agent into a bulk flow of material which has a chosen level of mixing and structuring.
It is also possible to control the shear (mixing) experienced by the materials after they have been combined, which can be used to manipulate the size of the benefit agent zones. The inventors have found that the benefit agent added by the process of the present invention can appear in the final detergent composition bar in non-spherical domains. In general, the domains are found to be elongate.
The bars produced containing substances, such as for example benefit agents, which are substantially immiscible with the detergent composition will essentially be two-phase systems. One phase may simply comprise the benefit agent, whilst the other phase comprises the detergent composition. Alternatively, the benefit agent may interact with one or more components of the detergent composition to form a separate benefit agent-containing phase.
Accordingly, in another aspect, the present invention provides a detergent bar obtainable by the process of the present invention, comprising detergent composition and components immiscible with the detergent compositions such as benefit agent, wherein the immiscible component is present in non-spherical domains. Other ingredients such as perfume or colourants may be introduced in the same way.
Benefit agents include components which moisturise, condition or protect the skin. Suitable benefit agents include moisturising components, such as, for example, emollient/oils. By emollient oil is meant a substance that softens the skin and keeps it soft by retarding the decrease of its water content and/or protects the skin.
Preferred benefit agents include:
Silicone oils, gums and modifications thereof such as linear and cyclic polydimethylsiloxanes; amino, alkyl, alkylaryl and aryl silicone oils. The silicone oil used may have a viscosity in the range 1 to 100,000 centistokes.
Fats and oils including natural fats and oils such as jojoba, soyabean, rice bran, avocado, almond, olive, sesame, persic, castor, coconut, mink, arachis, corn, cotton seed, palm kernel, rapeseed, safflower seed and sunflower oils; cocoa butter, beef tallow, lard; hardened oils obtained by hydrogenating the aforementioned oils; and synthetic mono, di and triglycerides such as myristic acid glyceride and 2-ethylhexanoic acid glyceride;
Waxes such as carnauba, spermaceti, beeswax, lanolion and derivatives thereof;
Hydrophobic plant extracts;
Hydrocarbons such as liquid paraffins, petrolatum, microcrystalline wax, ceresin, squalene and mineral oil;
Higher alcohols and fatty acids such as behenic, palmitic and stearic acids; lauryl, cetyl, stearyl, oleyl, behenyl, cholesterol and 2-hexadecanol alcohols;
Esters such as cetyl octanoate, cetyl lactate, myristyl lactate, cetyl palmitate, butyl myristate, butyl stearate, decyl oleate, cholesterol isostearate, myristyl myristate, glyceryl laurate, glyceryl ricinoleate, glyceryl stearate, alkyl lactate, alkyl citrate, alkyl tartrate, glyceryl isostearate, hexyl laurate, isobutyl palmitate, isocetyl stearate, isopropyl isostearate, isopropyl laurate, isopropyl linoleate, isopropyl myristate, isopropyl palmitate, isopropyl stearate, isopropyl adipate, propylene glycol monolaurate, propylene glycol ricinoleate, propylene glycol stearate, and propylene glycol isostearate;
Essential oils such as fish oils, mentha, jasmine, camphor, white cedar, bitter orange peel, ryu, turpentine, cinnamon, bergamont, citrus unshiu, calamus, pine, lavender, bay, clove, hiba, eucalyptus, lemon, starflower, thyme, peppermint, rose, sage, menthol, cineole, eugeniol, citral, citronelle, borneol, linalool, geraniol, evening primrose, camphor, thymol, spirantol, pinene, limonene and terpenoid oils;
Lipids such as cholesterol, ceramides, sucrose esters and pseudo-ceramides as described in EP-A-556 957;
Vitamins such as vitamin A and E, and vitamin alkyl esters, including those vitamin C alkyl esters;
Suncreens such as octyl methoxyl cinnamate (Parsol MCX) and butyl methoxy benoylmethane)Parsol 1789);
Phospholipids; and Mixtures of any of the foregoing components.
It should be understood that where the emollient may also function as a structurant, it should not be doubly included such that, for example, if the structurant is 15% oleyl alcohol, no more than 5% oleyl alcohol as xe2x80x9cemollientxe2x80x9d would be added since the emollient (whether functioning as emollient or structurant) should not comprise more than 20%, preferably no more than 15% by weight of the composition.
The emollient/oil is generally used in an amount from about 1 to 20%, preferably 1 to 15% by weight of the composition. Generally, it should comprise no more than 20% by weight of the composition.
The present invention will be further described by way of the accompanying drawings.